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Method for preparing flubendiamide

A technology of fluraniliprole and phthalamide, which is applied in the field of preparation of flubendiamide, can solve the problems of non-recyclable solvent, excessive waste acid, excessive waste acid, etc., and achieves low cost, reduction of waste acid, simple and safe operation Effect

Active Publication Date: 2013-03-27
SHANGHAI HETENG FINE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the solvent cannot be reused, and the waste acid is more
[0006] In summary, the above method produces more waste acid

Method used

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  • Method for preparing flubendiamide

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Effect test

Embodiment 1

[0016] 450 milliliters of DMF, 50 grams of concentration by weight are 95% nitric acid, 2 grams of manganese acetate and 66.6 grams (0.1 mole) of N2-[1,1-dimethyl-2-methanylethyl]-3-I- Add N1-[2-methyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethylethyl)phenyl]-1,2-benzenedicarboxamide into a 1000ml reaction flask , stirred and heated to 70° C., and air was introduced to carry out air oxidation. The reaction time was 8 hours, and the conversion of raw materials was greater than 99% by HPLC tracking. Recover DMF and nitric acid under reduced pressure, then add methanol and water for recrystallization. After drying, 60 g of product were obtained, a yield of about 88%.

Embodiment 2

[0018] 450 milliliters of DMF, 50 grams of concentration by weight are 95% nitric acid, 5 grams of manganese acetate and 66.6 grams (0.1 moles) of N2-[1,1-dimethyl-2-methylsulfonyl ethyl]-3-I -N1-[2-methyl 4-(1,2,2,2-tetrafluoro-1-trifluoromethylethyl)phenyl]-1,2-benzenedicarboxamide was added to a 1000 ml reaction flask , stirred and heated to 105° C., and air was introduced for air oxidation. The reaction time was 8 hours, and the conversion of raw materials was greater than 99% by HPLC tracking. Recover DMF and nitric acid under reduced pressure, then add methanol and water for recrystallization. After drying, 57 g of product were obtained, a yield of about 84%.

Embodiment 3

[0020] 400 milliliters of DMAC, 100 grams of 95% nitric acid, 2 grams of manganese acetate and 66.6 grams (0.1 moles) of N2-[1,1-dimethyl-2-methylsulfonylethyl]-3-I- Add N1-[2-methyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethylethyl)phenyl]-1,2-benzenedicarboxamide into a 1000ml reaction flask , stirred and heated to 90° C., air was introduced to carry out air oxidation, the reaction time was 5 hours, and the conversion of raw materials was greater than 99% by HPLC tracking. Recover DMAC and nitric acid under reduced pressure, then add methanol and water for recrystallization. After drying, 56 g of product were obtained, a yield of about 82%.

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Abstract

The invention provides a method for preparing flubendiamide. The method comprises the following steps of: adding N2-[1,1-dimethyl-2-methylmercaptoacylethyl]-3-I-N1-[2-methyl-4-(1,2,2,2-tetrachloro-1-trifluoromethaneethyl)-1,2-phthalic diamide to a solvent; introducing air in the presence of nitric acid and manganese acetate which are used as catalysts to carry out an oxidizing reaction; and then collecting a target product from a reaction product. In the method, because the air is used for carrying out the oxidizing reaction, the cost is reduced, and the acid is reduced; the raw material conversion can reach higher than 99 percent; and the method has the advantages of reasonable process, simple and safe operation, low cost and convenience for industrial production.

Description

technical field [0001] The invention relates to a preparation method of flubendiamide. Background technique [0002] Flubendiamide is a new type of phthalamide insecticide. Almost all lepidopteran pests have good activity. It not only has excellent activity against adults and larvae, but also has fast action speed and long-lasting effect. . It has special effects on rice stem borer and leaf roller. The toxicity to bees is very low, and the toxicity to carp (a representative of aquatic organisms) is also very low. It has no activity (virtually non-toxic) against beneficial insects at normal dosages. At present, there are mainly the following preparation methods: [0003] Document WO2005063703 discloses 2 -[1,1-Dimethyl-2-methylsulfonylethyl]-3-I-N1-[2-methyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethane Base ethyl) phenyl]-1,2-benzenedicarboxamide is the method that raw material obtains flubendiamide with hydrogen peroxide oxidation: [0004] [0005] Yield: 83-87%. In...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C317/28C07C315/02
Inventor 施冠成滑国钰蔡烨锋夏伟冬
Owner SHANGHAI HETENG FINE CHEM
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